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Preparation method for ammonium polyphosphate/polystyrene core-shell microspheres

A technology of ammonium polyphosphate and polystyrene, which is applied in the preparation of microspheres and microcapsule preparations, can solve the problems of difficult-to-modify ammonium polyphosphate, and the product of coated modified ammonium polyphosphate has no specific shape, and achieve toughness The effect of flame retardant modification integration, improved hydrophobic performance, and improved flame retardant durability

Active Publication Date: 2014-01-29
四川天策聚材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the coated modified ammonium polyphosphate product prepared by this method has no specific form, and it is difficult to obtain a modified ammonium polyphosphate with good reproducibility by adjusting the synthesis process.

Method used

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  • Preparation method for ammonium polyphosphate/polystyrene core-shell microspheres
  • Preparation method for ammonium polyphosphate/polystyrene core-shell microspheres
  • Preparation method for ammonium polyphosphate/polystyrene core-shell microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 20 parts by weight of ammonium polyphosphate, 0.5 parts of stabilizer and 50 parts of anhydrous methanol into a multi-port reaction kettle with reflux condensation device, thermometer and mechanical stirring. Add 5 parts of styrene monomer and 0.1 part of azobisisoheptanonitrile dropwise, wherein the styrene monomer and initiator are added dropwise at 0.5, and after continuing to react for 5 hours at 45°C, cool down to room temperature, filter, and use absolute ethanol for several times After washing, polydisperse ammonium polyphosphate-polystyrene core-shell microspheres with a particle size of about 1-3 μm are obtained. The transmission electron microscope image of the microsphere is attached figure 1 shown.

Embodiment 2

[0036] Add 20 parts by weight of ammonium polyphosphate, 1.75 parts of stabilizer and 120 parts of anhydrous methanol into a multi-port reaction kettle with a reflux condensation device, a thermometer and mechanical stirring. Add 60 parts of styrene monomer and 1.1 parts of azobisisobutyronitrile dropwise, wherein the styrene monomer and initiator are added dropwise at 0.5, continue to react at 70°C for 5 hours, cool down to room temperature, filter, and use absolute ethanol for several times After washing, polydisperse ammonium polyphosphate-polystyrene core-shell microspheres with a particle size ranging from 0.7 to 1.5 μm were obtained. The static contact angle test chart of the microsphere is attached image 3 Shown; the microspheres and pure ammonium polyphosphate and polystyrene thermogravimetric curve comparison chart as attached Figure 4 shown.

Embodiment 3

[0038]Add 20 parts by weight of ammonium polyphosphate, 0.7 parts of stabilizer and 80 parts of anhydrous methanol into a multi-port reaction kettle with a reflux condensation device, a thermometer and mechanical stirring. Add 20 parts of styrene monomer and 0.5 part of azobisisoheptanonitrile dropwise, wherein the styrene monomer and initiator are added dropwise at 0.5, and after continuing to react at 60°C for 3 hours, cool down to room temperature, filter, and use absolute ethanol for several times After washing, ammonium polyphosphate-polystyrene core-shell microspheres with a particle diameter of about 1.5 μm are obtained. The scanning electron microscope image of the microsphere is attached Figure 5 shown.

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Abstract

The invention discloses a preparation method for ammonium polyphosphate / polystyrene core-shell microspheres. The method is characterized by comprising the following steps: adding, by weight, 20 parts of ammonium polyphosphate, 0.5 to 5 parts of a stabilizer and 50 to 500 parts of a dispersion medium into a mechanically stirring multi-ported reaction vessel equipped with a reflux condensing unit and a thermometer; carrying out ultrasonic wave-assisted mechanical stirring so as to uniformly mix the above-mentioned substances; simultaneously adding 5 to 100 parts of styrene monomers and 0.1 to 2 parts of an initiator into the reaction vessel drop by drop, wherein addition of the styrene monomers and the initiator is finished within 0.5 to 1.5 h; and continuing a reaction at a temperature of 45 to 80 DEG C for 1 to 5 h, allowing temperature to drop to room temperature and carrying out filtering and washing so as to obtain the core-shell microspheres with diameters of 0.1 to 3 mu m. The ammonium polyphosphate / polystyrene core-shell microspheres prepared by using the method provided by the invention has a controllable particle size, excellent thermal stability and a plurality of functions like toughening performance, flame-retardation and hydrophobicity and can be used for toughening and flame-retardation modification of thermosetting resins like benzoxazine.

Description

technical field [0001] The invention relates to a method for preparing multifunctional core-shell microspheres with ammonium polyphosphate as the core and polystyrene as the shell, belonging to the field of multifunctional modification of halogen-free flame retardants. Background technique [0002] Ammonium polyphosphate is also called ammonium polyphosphate or polycondensed ammonium phosphate (Ammonium polyphosphate, APP), and its general molecular formula is (NH 4 ) (n+2) P n o (3n+1) , wherein, when n is 10~20, it is water-soluble; when n is greater than 20, it is insoluble. Ammonium polyphosphate is non-toxic and tasteless, does not produce corrosive gas, has a phosphorus content of 30%~32%, and a nitrogen content of 14%~16%. It has a good flame retardant effect and has been widely used in polymer materials. combustion modification. However, there are a large number of P-O-P and P=O bonds in the molecular structure of ammonium polyphosphate, which leads to its stron...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K3/32C08F112/08C08L79/04B01J13/14
Inventor 李云涛赵春霞邢云亮
Owner 四川天策聚材科技有限公司